تفاعل #77409
ord-b8a314062fdf4bcab30d98bf959af708
معادلة التفاعل
4-methoxyphenylboronic acid
5-bromo-2-fluoronitrobenzene
sodium carbonate
→
4-fluoro-4′-methoxy-3-nitrobiphenyl
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةThe mixture was heated
- 2درجة الحرارةto reflux for 2 hours
- 3تركيزconcentrated
- 4استخلاصthe residue extracted twice with ethyl acetate
- 5غسيلThe ethyl acetate layer was washed with water, brine
- 6أخرىdried
- 7تركيزconcentrated
- 8أخرىto give a brown oily solid
- 9أخرىThe solid was purified by column chromatography on silica gel in 5% ethyl acetate in hexane
الإجراء التجريبي
Tetrakis(triphenylphosphine)palladium (1 g) was added to a mixture of 5 g of 4-methoxyphenylboronic acid, 6.6 g of 5-bromo-2-fluoronitrobenzene and 30 mL of 2M sodium carbonate solution in 50 mL of toluene and 50 mL of ethanol. The mixture was heated to reflux for 2 hours, concentrated, and the residue extracted twice with ethyl acetate. The ethyl acetate layer was washed with water, brine, dried, and concentrated to give a brown oily solid. The solid was purified by column chromatography on silica gel in 5% ethyl acetate in hexane to give crude-4-fluoro-4′-methoxy-3-nitrobiphenyl as a pale yellow solid.